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Additive-free continuous synthesis of silica and ORMOSIL micro- and nanoparticles applying a microjet reactor

  • Original Paper: Sol-gel, hybrids and solution chemistries
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A Correction to this article was published on 20 January 2020

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Abstract

The continuous wet chemical preparation of micro- and nanoparticles is a major challenge for the large-scale production of functional colloids. Here we present a general synthetic strategy for sol–gel-based materials via an additive free homogenous approach avoiding emulsion-based systems. A variety of different silica and organically-modified silica (ORMOSIL) spherical particles were prepared applying a condensation of prehydrolyzed alcoholic solution of organotrialkoxysilanes in a microjet reactor. This method presents a unique wet chemical production method for nano- and microscale materials. Methyl-, ethyl-, propyl-, vinyl-, phenyl-, and mixed ORMOSIL particles in the range of 75 nm–2 µm were successfully synthesized without the addition of stabilizing surfactants. The method was also investigated for the continuous preparation of pure silica particles, and we succeeded to produce continuously up to 23 g particles per minute. The influence of different organic groups on the crosslinking of the siloxane network was systematically studied applying various spectroscopic and thermoanalytical methods. The degree of condensation of the obtained particles depends on the organic rests of the trialkoxysilanes, which was studied with 29Si CP-MAS NMR. We were able to show that phenyl silsesquioxanes show less condensation in the particles than smaller alkyl or vinyl groups. In addition, the silane concentration has a significant influence on the particle size. Generally, smaller particle diameters are obtained after decreasing the silane concentration. The described process delivers a fast and large scale wet chemical production of various silsesquioxane and silica particles without the use of additives and is therefore suited for a variety of potential applications where high purity of the particles is necessary.

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Change history

  • 20 January 2020

    An amendment to this paper has been published and can be accessed via a link at the top of the paper.

  • 20 January 2020

    An amendment to this paper has been published and can be accessed via a link at the top of the paper.

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Acknowledgements

We thank Dr. Michael Zimmer for the CP-MAS-NMR measurements and Susanne Harling for elemental analyses.

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Authors and Affiliations

  1. Saarland University, Inorganic Solid State Chemistry, Campus, Building C4 1, 66123, Saarbrücken, Germany

    Christina Odenwald & Guido Kickelbick

Authors
  1. Christina Odenwald
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  2. Guido Kickelbick
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Correspondence to Guido Kickelbick.

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The authors declare that they have no conflict of interest.

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Highlights

  • The paper shows for the first time the continuous, wet chemical preparation of ORMOSIL micro-and nanoparticles applying a microjet reactor.

  • No additives for the stabilization of the particles are required.

  • The particles can be prepared with yields up to 23 g min−1.

  • Well-defined particle morphologies were obtained of methyl-, ethyl-, propyl-, vinyl-, and phenyl-ORMOSILs as well as pure silica particles.

  • The condensation degrees of the particles vary depending on the organic substitution pattern at the silicon atom.

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Odenwald, C., Kickelbick, G. Additive-free continuous synthesis of silica and ORMOSIL micro- and nanoparticles applying a microjet reactor. J Sol-Gel Sci Technol 89, 343–353 (2019). https://doi.org/10.1007/s10971-018-4626-x

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  • DOI: https://doi.org/10.1007/s10971-018-4626-x

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